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WO2004004890A1 - Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it - Google Patents

Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it Download PDF

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Publication number
WO2004004890A1
WO2004004890A1 PCT/GE2002/000008 GE0200008W WO2004004890A1 WO 2004004890 A1 WO2004004890 A1 WO 2004004890A1 GE 0200008 W GE0200008 W GE 0200008W WO 2004004890 A1 WO2004004890 A1 WO 2004004890A1
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WIPO (PCT)
Prior art keywords
diatomite
powder
ultrafiltering
production
mkm
Prior art date
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Ceased
Application number
PCT/GE2002/000008
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French (fr)
Inventor
Irakli Grishashvili
Irakli Menabde
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Individual
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Individual
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Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to AU2002314394A priority Critical patent/AU2002314394A1/en
Priority to PCT/GE2002/000008 priority patent/WO2004004890A1/en
Publication of WO2004004890A1 publication Critical patent/WO2004004890A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/16—Use of materials for tobacco smoke filters of inorganic materials
    • A24D3/166—Silicic acid or silicates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3035—Compressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing

Definitions

  • the present invention refers to the method of production of absorbent from diatomite and technology of production of ultrafilter powder materials required for food industry and may be also used in production of pure liquids, gases and cigarette filters.
  • activated charcoal as the absorbent is widely used in cigarette filters along with the acetate paper filters [SEKAP S.A. Products Table, http://www.sekap.grl5.12.1999 Greek Cooperative Cigarette Manufacturing Company S.A].
  • the activated charcoal is placed between two acetate filters and act as the absorbent, but it fails to meet the requirements as cannot catch the multicycle aromatic hydrocarbons and nitrose compounds harmful for human health.
  • the proposed invention ensures obtaining of ultrafiltering powder material from diatomite for production of membrane filters with homogenous distribution of pores and equal thickness and manufacturing of cigarette membrane filters from it.
  • the technical result of the invention is increase in the assortment of the filtering material.
  • the method provides fracturing of diatomite basic material, drafting at high temperature, mixing of modifier, grinding, sieving, at the same time the diatomite powder grains of size not exceeding 5 mm shall be burnt out at 850°C in the atmospheric conditions during 2 hours.
  • the diatomite powder is mixed with 5 mass-percent of table salt powder and matured at the mentioned temperature for 10 minutes whereupon it is cooled at the room temperature.
  • the obtained powder with the dispersity of particles 0.5-5 mkm is grounded by pressure to the thickness of 0.1-1 mkm in the form of the ultrafilter with the homogenous distribution of pores.
  • the cigarette filter with the front and back acetate filters and the ultrafiltering material placed between them is produced according to the above-mentioned method.
  • Example 1 The cigarette filter with the front and back acetate filters and the ultrafiltering material placed between them is produced according to the above-mentioned method.
  • the diatomite basic material (white diatomite from Kasatibi deposit, Georgia) fractured into 1-5 mm particles is placed into the furnace where it is burned at 850° C in the air conditions during 2 hours.
  • the diatomite powder is mixed with 5 mass-percent of table salt powder with the dispersity of particles 0.05-05 mm (which conforms to the former USSR standards GOST-13830-91).
  • the mixture shall be cooled along with the furnace up to the room temperature, ground in the planetary grinder or any other grinding machine and then through the sieving they obtain the powdery material with the specific morphology of porous, plate perimeter- notched particles of 0.5-5 mkm size.
  • Those particles by a slight pressing can be easily structured on the filter holder in the form of ultrafilters (membrane - filters) with homogenous distribution of pores of 0.1-1 mkm sizes.
  • the diatomite powder catches nicotine by 5% and the tar - by 15 % better than the activated charcoal. In addition the diatomite powder catches the multicycle aromatic hydrocarbons and nitrose compounds.
  • the scanning electromicroscopic and X-ray study of the materials obtained at each stage of the cycle according to the invention was carried out.
  • the study by this method was carried out on the basic material - diatomite produced on the Kasatibi deposit.
  • the X-ray study showed that its chemical composition by 96% consists of opal (Si0 2 nH 2 0) and it remains stable at any temperature and in other processing conditions provided for by the invention.
  • Fig. la shows the scanning electromicroscopic image of white diatomite powder taken as the raw material in the secondary electronic detection.
  • the statistic analysis showed that the diatomite basic material (Ethmodicus gazellae) by 85-90 % consists of siliceous coats of flap type with radial cuts as shown on Fig. 1, the diameter of which varies from 4 mkm to 10 mkm.
  • the basic material in addition to the main type coats contains two more types of diatomite: Gyrosigma atteniatum (Fig. lb) and Surirela robusta (Fig. Ic) of 10-12 % total quantity.
  • Fig. la contains two more types of diatomite: Gyrosigma atteniatum (Fig. lb) and Surirela robusta (Fig. Ic) of 10-12 % total quantity.
  • Fig. la contains two more types of diatomite: Gyrosigma atteniatum (Fig. lb) and Surirela robusta (Fig. Ic) of 10-12 % total quantity.
  • Fig. la The basic material in addition to the main type coats (Fig. la) contains two more types of diatomite: Gyrosigma atteniatum (Fig. lb) and Surirela robusta (Fig. Ic) of 10-12 % total quantity.
  • Fig. Ic Surirela robusta
  • Fig. 2a and Fig. 2b respectively give the electromicroscopic images of untreated diatomite powder pressed by 5kg/cm force and the diatomite powder treated by the table salt pressed by the same force.
  • the later image in turn confirms that the diatomite powder obtained in accordance to the invention is the best material for production of an ultrafilter with the homogenous distribution of pores of 0.1-1 mkm with the desired thickness through grinding by pressure on the filter holders.
  • 1 the curve for the activated carbon used in the prototype cigarette filter.
  • the curve is resulted from the experimental data obtained by the method of mercury drafting; 2 - the curve for non-treated diatomite from Kisatibi deposit (sieved after grinding); 3 - the curve for the ultrafiltering material obtained from diatomite by the present invention.
  • the ultrafiltering material proposed by the invention distinguishes by the monomodal nature of distribution according to the effective radiuses of pore volume, the pique of which is arranged at the lower bound of the porous sorbent range for the pores of 2500 A diameter, while for the activated carbon two piques are typical: one for the maximum number of pores of 200 A diameter at the lower bound of range of the transitional porous sorbent, and the second pique for the less number (twofold) of pores at the upper bound of the porous sorbent range of 1/5 mkm diameter.
  • Still another advantage of the invention is that the replacement of the sorbent - the activated charcoal used in the cigarette filters with the ultrafiltering material obtained by the proposed method will enable creation of the new membrane filter with the advanced filtering qualities.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The method provides for fractionating of diatomite raw material, its burning out at high temperature, adding of modifier, grinding, sieving, wherein the diatomite powder with the size of grains not exceeding 5 mm shall be calcined at 850°C at atmospheric conditions during 2 hours and the diatomite powder mixing with table salt powder at 5 % mass-percent and then matured at the said temperature for 10 minutes whereupon it is cooled to room temperature. The produced powder with particles of 0.5-5 µm size is ground by pressure to the desired thickness in the form of a (membrane) ultrafilter with a homogenous distribution of pores of size 0.1-1 µm. The cigarette filter containing the front and back acetate filters with the ultrafiltering material between them is produced by the above-mentioned method.

Description

METHOD OF PRODUCTION OF A DIATOMITE ULTRAFILTERING MATERIAL AND CIGARETTE MEMBRANE FILTER COMPRISING IT
The present invention refers to the method of production of absorbent from diatomite and technology of production of ultrafilter powder materials required for food industry and may be also used in production of pure liquids, gases and cigarette filters.
It is known the method of production of filtering materials, which provides for selection of filtering materials chemically neutral to liquids and gases, achievement to the required porosity of them (pore size and number), obtaining of powders of the specified dispersivity and then formation of filters on flexible or hard holders. [SU 1526813 Al Bull. N<> 45, 07.12.1989]
. Notwithstanding the great demand the assortment of easily pressed homogenous porous dispersive materials is still rather limited to date.
It is known the method of production of absorbent without any binding agent [SU 1526813 Al Bull. JSfe 45, 07.12.1989]. However, this method could not provide formation of ultra-filters of the equal thickness and homogenous distribution of pores for production of ultra-filters (membrane filters) required for ultrafiltering processes.
It is also known that the activated charcoal as the absorbent is widely used in cigarette filters along with the acetate paper filters [SEKAP S.A. Products Table, http://www.sekap.grl5.12.1999 Greek Cooperative Cigarette Manufacturing Company S.A]. The activated charcoal is placed between two acetate filters and act as the absorbent, but it fails to meet the requirements as cannot catch the multicycle aromatic hydrocarbons and nitrose compounds harmful for human health.
The proposed invention ensures obtaining of ultrafiltering powder material from diatomite for production of membrane filters with homogenous distribution of pores and equal thickness and manufacturing of cigarette membrane filters from it.
The technical result of the invention is increase in the assortment of the filtering material.
The method provides fracturing of diatomite basic material, drafting at high temperature, mixing of modifier, grinding, sieving, at the same time the diatomite powder grains of size not exceeding 5 mm shall be burnt out at 850°C in the atmospheric conditions during 2 hours. At the same temperature, the diatomite powder is mixed with 5 mass-percent of table salt powder and matured at the mentioned temperature for 10 minutes whereupon it is cooled at the room temperature. The obtained powder with the dispersity of particles 0.5-5 mkm is grounded by pressure to the thickness of 0.1-1 mkm in the form of the ultrafilter with the homogenous distribution of pores.
The cigarette filter with the front and back acetate filters and the ultrafiltering material placed between them is produced according to the above-mentioned method. Example 1.
The diatomite basic material (white diatomite from Kasatibi deposit, Georgia) fractured into 1-5 mm particles is placed into the furnace where it is burned at 850° C in the air conditions during 2 hours. At the same temperature the diatomite powder is mixed with 5 mass-percent of table salt powder with the dispersity of particles 0.05-05 mm (which conforms to the former USSR standards GOST-13830-91). After 10-minute allowance following the completion of mixing the mixture shall be cooled along with the furnace up to the room temperature, ground in the planetary grinder or any other grinding machine and then through the sieving they obtain the powdery material with the specific morphology of porous, plate perimeter- notched particles of 0.5-5 mkm size. Those particles by a slight pressing can be easily structured on the filter holder in the form of ultrafilters (membrane - filters) with homogenous distribution of pores of 0.1-1 mkm sizes. Example 2.
We have taken cigarette "BF" (Greece) with the removed activated charcoal powder placed between the front and back acetate filters. In place of the charcoal we have put the diatomite powder layer 2 mm thickness with dispersity of 0.1-0.5 mkm.
By nicotine and tar testing it was determined that the diatomite powder catches nicotine by 5% and the tar - by 15 % better than the activated charcoal. In addition the diatomite powder catches the multicycle aromatic hydrocarbons and nitrose compounds.
The scanning electromicroscopic and X-ray study of the materials obtained at each stage of the cycle according to the invention was carried out. In the first turn the study by this method was carried out on the basic material - diatomite produced on the Kasatibi deposit. The X-ray study showed that its chemical composition by 96% consists of opal (Si02nH20) and it remains stable at any temperature and in other processing conditions provided for by the invention.
Fig. la shows the scanning electromicroscopic image of white diatomite powder taken as the raw material in the secondary electronic detection. The statistic analysis showed that the diatomite basic material (Ethmodicus gazellae) by 85-90 % consists of siliceous coats of flap type with radial cuts as shown on Fig. 1, the diameter of which varies from 4 mkm to 10 mkm.
The basic material in addition to the main type coats (Fig. la) contains two more types of diatomite: Gyrosigma atteniatum (Fig. lb) and Surirela robusta (Fig. Ic) of 10-12 % total quantity. As it is seen on the given image such diatomite components represent by themselves the best porous ultrafilters. However, grinding and pressing of this material do not give us the desirable result in terms of obtaining the homogenous ultrafilter (membrane filter) of the equal thickness.
Fig. 2a and Fig. 2b respectively give the electromicroscopic images of untreated diatomite powder pressed by 5kg/cm force and the diatomite powder treated by the table salt pressed by the same force. The later image in turn confirms that the diatomite powder obtained in accordance to the invention is the best material for production of an ultrafilter with the homogenous distribution of pores of 0.1-1 mkm with the desired thickness through grinding by pressure on the filter holders.
Calculation of geometrical and sorptive parameters of pores between the particles of ultrafiltering material from diatomite and the prototype activated charcoal on the basis of experimental data obtained by the scanning electronic microscope shows that the technical results achieved by the invention are mainly conditioned by the morphological and structural qualities of the used diatomite particles and the pores existing inside. Fig. 3 shows the differential curves of distribution according to the effective radiuses (diameters) of the pore amount:
1 - the curve for the activated carbon used in the prototype cigarette filter. The curve is resulted from the experimental data obtained by the method of mercury drafting; 2 - the curve for non-treated diatomite from Kisatibi deposit (sieved after grinding); 3 - the curve for the ultrafiltering material obtained from diatomite by the present invention.
It is obvious that unlike the activated carbon, the ultrafiltering material proposed by the invention distinguishes by the monomodal nature of distribution according to the effective radiuses of pore volume, the pique of which is arranged at the lower bound of the porous sorbent range for the pores of 2500 A diameter, while for the activated carbon two piques are typical: one for the maximum number of pores of 200 A diameter at the lower bound of range of the transitional porous sorbent, and the second pique for the less number (twofold) of pores at the upper bound of the porous sorbent range of 1/5 mkm diameter.
As the calculation has shown, for cigarette filter it will be required two- times less quantity (in grams) of sorbent proposed by the given invention ascompared with the activated charcoal use in the prototype. Therefore, those skilled in the art could easily understand that use of ultrafiltering material obtained in the basis of the invention for production of the cigarette membrane filter will enable reduction of the thickness of sorbent layer placed between the front and back acetate filters of the cigarette about two-times.
Still another advantage of the invention is that the replacement of the sorbent - the activated charcoal used in the cigarette filters with the ultrafiltering material obtained by the proposed method will enable creation of the new membrane filter with the advanced filtering qualities.

Claims

Claims
1. A method for production of an ultrafiltering material comprising the steps of fracturing squeezing, burning at high temperature, modifier mixing, grinding and sieving of the diatomite basic material characterized in that the diatomite powder with grains not exceeding 5 mm is burned out at 850 ° C in the air conditions during 2 hours with mixing of the table salt powder at 5% mass-percent, kept at the mentioned temperature for 10 minutes and then cooled up to the room temperature along with the furnace, the produced powder with particles of 0.5-5 mkm dispersity being pressed on the filter holder at the equal thickness 0.1-1 mkm in the form of the ultrafilter of homogenous pore distribution.
2. The cigarette membrane filter including front and back acetate filters with the adsorbent powder layer between them characterized in that the filter as the absorbent contains the ultrafiltering material produces according to the method of claim 1.
PCT/GE2002/000008 2002-07-08 2002-07-08 Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it Ceased WO2004004890A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2002314394A AU2002314394A1 (en) 2002-07-08 2002-07-08 Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it
PCT/GE2002/000008 WO2004004890A1 (en) 2002-07-08 2002-07-08 Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it

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PCT/GE2002/000008 WO2004004890A1 (en) 2002-07-08 2002-07-08 Method of production of a diatomite ultrafiltering material and cigarette membrane filter comprising it

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1868576B (en) * 2005-05-24 2010-10-27 黄亮 Biologically modified diatomite adsorbent and preparation method thereof
CN109222220A (en) * 2018-08-30 2019-01-18 龙岩烟草工业有限责任公司 For evaluating and testing the method and system of cigarette manufacturing quality index
CN116943604A (en) * 2023-07-10 2023-10-27 云南中烟工业有限责任公司 Modified diatomite as well as preparation method and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1502547A (en) * 1922-11-06 1924-07-22 Calvert Robert Diatomaceous earth product and process of making the same
GB229021A (en) * 1923-11-22 1925-02-19 Celite Company Treatment of diatomaceous earth
US1826331A (en) * 1927-06-23 1931-10-06 Traube Isidor Method of doing away with the nicotine and the methylalcohol when smoking tobacco
CH488413A (en) * 1968-02-01 1970-04-15 Ed Laurens S A Cigarette filter
US3608563A (en) * 1969-02-06 1971-09-28 John B Schmitz Cigarette filter

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1502547A (en) * 1922-11-06 1924-07-22 Calvert Robert Diatomaceous earth product and process of making the same
GB229021A (en) * 1923-11-22 1925-02-19 Celite Company Treatment of diatomaceous earth
US1826331A (en) * 1927-06-23 1931-10-06 Traube Isidor Method of doing away with the nicotine and the methylalcohol when smoking tobacco
CH488413A (en) * 1968-02-01 1970-04-15 Ed Laurens S A Cigarette filter
US3608563A (en) * 1969-02-06 1971-09-28 John B Schmitz Cigarette filter

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1868576B (en) * 2005-05-24 2010-10-27 黄亮 Biologically modified diatomite adsorbent and preparation method thereof
CN109222220A (en) * 2018-08-30 2019-01-18 龙岩烟草工业有限责任公司 For evaluating and testing the method and system of cigarette manufacturing quality index
CN109222220B (en) * 2018-08-30 2021-08-20 龙岩烟草工业有限责任公司 Method and system for evaluating cigarette rolling quality index
CN116943604A (en) * 2023-07-10 2023-10-27 云南中烟工业有限责任公司 Modified diatomite as well as preparation method and application thereof
WO2025010772A1 (en) * 2023-07-10 2025-01-16 云南中烟工业有限责任公司 Modified diatomite, and preparation method therefor and use thereof

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